Coloration of textile materials



Patented Dec. 22, 1942 COLORATION 0F TEXTILE MATERIALS George Schneider, Montclair, N. J., assignor to of America, a corporation Celanese Corporation of Delaware No Drawing. Application March 19, 1940,

' Serial No. 324,797 I 8 Claims.

Thisinvention relates to the coloration of textile materials, and relates more particularly to the production of dark colors on textile materials made of or containing cellulose esters or ethers- This invention is a continuation-in-part of the invention described in application S. No. 277,619 filedJune 6, 1939. I

An important object of this invention is. the

' economic and expeditious production of an artificial material having a neutral grey color which is fast to light, acid and perspiration.

I Another object of this invention is the production of an artificial textile material which is neutral grey in color and which is free from red, brown or blue fluorescence or cast. a

A further object of this invention is the production with greater ease and at less expense of fast dark shades on textile materials made of or containing cellulose esters or ethers by dyeing the neutral grey colored materials, produced in accordance with thi invention,- by direct dyeing methods.

as compared with those usually suflicient for the production of pale or medium shades. As a consequence the deep dyeings produced by direct dyeing methods frequently lack fastness to rubbing in addition to lacking fastness to other agencies. Furthermore, the use of such high pro portions of coloring matters involves considerable expense. Consequently, if satisfactory deep shades are required, it has generally been found expedient to employ indirect dyeing methods such as dyeing with vat dyestufis or with azo dyestufis produced on the material. These latter methods, however, suffer from the grave disadvantage that they require exceptional skill and that the matching of shades to a given sample is a mater of some difliculty.

The aforesaid difliculties are particularly pronounced in the case of cellulose ester or ether materials owing to the substantial absence of any direct dyeing unitary dyestuffs capable of yielding black or other dark shades thereon. If,

therefore, it is desired to produce such dark shades by direct dyeing methods, it has been essential to employ very large proportions of mixtures of brightly dyed dyestuffs. Thus, black shades have been produced by the application of a mixture of direct dye blue, red and orange or yellow dyestuffs in which the blue predominates.

Such dyeings are particularly prone to lack fastness to rubbing.

It has been proposed to incorporate in textile materials a dark colored pigment of such character and in such proportion as to yield thereon a grey, drab or other dark shade and then subsequently dyeing these materials by direct dyeing methods to produce a wide range of colors using only relatively small quantities of direct dyeing dyestuffs. I have now found that very satisfactory deep dark shades may be produced on materials made of or containing cellulose esters or ethers by incorporating in the materials black dyestuffs. These dyestuffs give to the material a desirable neutral shade free from red, brown or blue fluorescence or cast. When'such neutral grey colored materials are dyed with direct'dyeing dyestuffs, deep dark shades which are fast to rubbing are produced. In accordance with my invention, therefore, I produce textile materials having a neutral grey shade by incorporating in said textile materials a small amount of a mixture of black dyestuffs, preferably a mixture of Aniline Black and Alizarin Cyanine Black (Colour Index No. 1065).

Dark shades are produced on the textile materials colored neutral grey in accordance with this invention by dyeing the same with dyestuffs having an affinity for the textile materials. accordance with the process of this invention, a reduced amount of the direct dyeing dyestuff is necessaryto produce desirabledeep dark shades on the textile materials. 'Furthermore, the incorporation of the dyestuffs in the material is particularly easy as the operation may readily be effected by way of the spinning solution from which the materials are produced. This method is of particular value in the production of dark shades upon artificial filaments or yarns of cellulose esters or ethers for, as indicated above, there is for these materials a marked lack of direct dyeing dyestufis inherently capable of yielding deep shades thereon.

'I'he grey neutral shades produc'ed in aocord-' ance with this invention are of particular value in that by applying relatively small quantities of dyestuffs thereto an extremely wide range of deeply colored material maybe produced from corporated therein. Thus, in order to produce black shades small amounts only of blue, red andyellow need be applied to the neutral grey material. Moreover, by an application to the same neutral grey material of green or a mixture of blue and yellow dyestuffs there may be produced a series of olive green, khakis, drabs and the like. Where yellows, oranges and reds are applied to the neutral green materials shades varying from yellow brown to chocolate may be obtained, while purple,rviolet and the like produce wine shades such as, for example, Bordeaux, maroon, etc.

It will be appreciated from theforegoing that for commercial requirements it is not essential, in order to obtain a satisfactoryrange of deep shades, to manufacture more than a very limited number of neutral grey materials. In fact, two or three materials having difierent amounts of Alizarin Black dyestuffs therein will be found to be sufiicient to cover practically all commercial requirements as regards dark shades.

As previously indicated, myinvention is of particular importance in connection with the-production of deeply colored cellulose ester or ether material, more particularly on account; of the lack of inherently dark dyestufis for these materials. As examples of such cellulose esters or ethers, especial mention maybe made of cellulose acetate and of other organic acid esters of cellulose, for example, cellulose propionate and cellulose butyrate, also ethers of cellulose, e. g, ethyl cellulose and benzyl cellulose. My invention is not, however, limited to the treatment or production of cellulose ester or ether textile materials in the form of filaments or yarns, as it may be applied to cellulose esters or ethers in other formssuch as, for example, ribbons, straws or films or like productsv having a large surface in relation to their mass. The process of my invention may also be applied to textile materials generally either natural or artificial, and especially to such artificial materials as may be prepared by extrusion of appropriate solutions, for example, regenerated cellulose prepared from viscose, and synthetic linear polyamide condensation products such as the polyamides derived from amino-acids or from the condensation products of diamines with carboxylic acids,'e. g. polyhexamethylene adipamide.

As previouslyindicated,I prefer to use a mixture of Aniline Black and Alizarin Cyanine Black.

While these substances may be incorporated in the materials at any stage of production of the latter, I prefer to incorporate the same in the ous filtration is spun into filaments by a dry spintion other than that supplied'by the candle and jet of the spinningapparatus may be eliminated.

In forming the neutral grey colored filaments or yarn there is employed in the spinning solution from 0.3 to 0.9%, and preferably 0.7% based on the weight of the cellulose acetate present, of black dyestuffs. However, lesser or larger amounts may be employed where desired.

In order further to illustrate my invention, but

. without being limited thereto the followingspecific examples are given.

Example I '20 parts by weight of a mixture of Aniline Black and Alizarin Cyanine Black in powder form is added to a solution containing 40 parts'by weight of cellulose acetate dissolved in 360 parts by weight. of acetone and the resulting mixture is milled for twenty-four (24) hours in a ball mill. A cellulose acetate spinning solution containing 25% of cellulose acetate dissolved in acetone is then prepared. Tothis spinning solution is added sufilcient of the above dyestufi dispersion to give a dyestufl concentration therein of 0.7% based on the weight of the cellulose acetate. The spinning solution containing the dyestufl without extranening process, producing yarns of a neutral grey color. The neutral grey colored yarns are free from a red, brown, or blue cast and,are found to be of substantially the same physical characteristics as those obtained by spinning a solution which is free from the dyestufls;

Example II The neutral grey yarn obtained by the process of Example I is dyed from a 30 to 1 soap bath containing dispersed therein coloring matters having direct afiinity for the cellulose acetate. The yarn is entered into the bath ata relatively low temperature which is gradually increased .to 70 to 80 -C. and the dyeing continued until the desired shadev is achieved. The yarn is then withdrawn from the dye bath, washed, dried and finished in the usual manner. Any of the direct dyeing dyestuffs having 'afilnity' for the cellulose .to secure by Letters Patent is:

spinning solution from which the filaments of cellulose esters or ethers are spun. The dyestuf! mixture or dispersion containing the black dye-'- stuifs which is to be added to the spinning solution is prepared by grinding, rubbing or-kneading'the dyestuffs in the presence of a derivative of cellulose and a solvent therefor. In this manner the dyestuffs are ground to' relatively fine particle size. For example, Alizarin Black dyestuffs, preferably in the form of powders, may be ground in the presence of cellulose acetate dissolved in acetone. The mixture or dispersion so formed has a dyestufi concentration of from 1 to 50%. based on the weight of the cellulose acetate presthe viscosity of the cellulose acetate employed. The grinding of the dyestuffs in the presence of the cellulose derivative and solvent produces a ent, the amount of dyestufi depending in part-on dyestufi particle size of such fineness that filtrall acetate may be employed.

It is to be understood that the foregoing detailed description is given merely by way of illustration and that many variations may bemade therein without departing from the spirit of my invention.

Having described my invention, what I desire 1. A solution for use in the manufacture of neutral grey colored filaments by extruding the same into a setting medium, comprising a cellulose derivative selected from the group consisting of cellulose 'esters and ethers dissolved in a solvent therefor and containing a. dispersion of a mixture of Aniline Black and Alizarin Cyanine Black. 2. A solution for use in the manufacture of neutral grey colored filaments by extruding the same into a setting medium, comprising a cellulose acetate dissolved in a solvent therefor and containing a dispersion of a mixture of Aniline Black and Alizarin Cyanine Black.

3. A solution for use in the manufacture of neutral grey colored filaments by extruding the same into a setting medium, comprising a cellua Black in an amount sufilcient to give a concentration of between 0.3 and 0.9%, based on the weight of the cellulose derivative present in the solution. 7

4. A solution for use in the manufacture of neutral grey colored filaments by extruding the same into a setting medium, comprising a cellumixture of Aniline Black and Alizarin Cyanine Black in an amount suflicient to give a 0.7% concentration.-

6. A solution for use in the manufacture of neutral grey colored filaments by extruding the same into a setting medium, comprising a cellulose acetate dissolved in a solvent therefor andcontaining a dispersion of a mixture of Aniline Black and Alizarin Cyanine Black in an amount sufficient to give a 0.7 concentration.

'7. Neutral'grey colored textile materials comprising materials having abasis of a cellulose derivative selected from the group consisting of cellulose esters and ethers and having incorporated therein a mixture of Aniline Black and Alizarin Cyanine Black.

8. Neutral grey colored textile materials comprising materials having a basis of cellulose acetate andhaving incorporated therein a mixture of Aniline Black and Alizarin Cyanine Black.

GEORGE SCHNEIDER. 

